The scattered field from an object, when illuminated with ultrasound, is useful in the reconstruction of it's cross section - a problem broadly classified as 'tomography'. In many situations of medical imaging, we will be interested in getting to know the location and the extent of growth of the inhomogeneity. The Maximum Likelihood (ML) estimation of the location and the shape parameters (of scale and orientation angle), has been done along with the corresponding CR bounds, for the case of weakly scattering objects, where the Fourier Diffraction Theorem(FDT) holds. It has been found that the a-priori information of a reference object function helps in drastic reduction of the number of receivers and illuminations required. For a polygonal object, the shape is specified, when the corner locations are known. We have formulated the problem as, estimation of the frequencies of sum of undamped sinusoids. The result is a substantial reduction in the number of illuminations and receivers required. For acoustically soft and rigid polygons, where the FDT does not hold, the necessary theory is developed to show the dependence of the scattered field on the corner location, using an On Surface Radiation Condition(OSRC). The corner locations are estimated along similar lines, to the one adopted for the weakly scattering objects.

This thesis is concerned with the evaluation, in-situ, of the elastic strain energy release rate of cracks. This can define the criteria for crack propagation, and it is usually necessary to obtain this via calculation from the geometry and applied load. A new method is proposed, based on the conjoint use of digital image correlation to measure full-field displacements and finite element to extract the strain energy release rate of surface cracks. It has been extended to 3-D datasets with the use of digital volume correlation and tomographic imaging. A finite element model with imported full-field displacements measured by DIC/DVC acting as boundary conditions is solved and the J-integral is calculated. For linear elastic materials, modal contributions can be separated via the interaction integral. The method has been benchmarked using synthetic datasets to assess its sensitivity to noise and experimental uncertainties. It is very robust to experimental noise and can be used without knowledge of the specimen geometry and applied loads. The application of the method in 2-D is demonstrated in an analysis of experimental data for a mode I fatigue crack, introduced to an aluminium alloy compact tension specimen. Analysis of mixed-mode cracks in 2-D is shown on a PMMA sample with the Arcan geometry. In 3-D, static loading of a fatigue crack in nodular graphite cast iron is studied and the results from the method are compared with those obtained via a field-fitting approach. Diffraction analysis of polycrystalline materials can determine the full tensor of the elastic strains within them. Maps of elastic strains can thus be obtained typically using synchrotron X-rays or neutrons. A method is presented to calculate the elastic strain energy release rate of a crack from 2-D diffraction strain maps. The diffraction data is processed via a finite element approach to obtain the parameters required to calculate the $J$-integral. A validation is presented using a synthetic dataset from a finite element model. Its experimental application is demonstrated in an analysis of synchrotron X-ray diffraction strain maps of a propagating fatigue crack in a bainitic steel, before and after an overload. Finally, a complex case study of stable fracture propagation in polygranular isotropic nuclear graphite is presented. Synchrotron X-ray tomography and strain mapping by diffraction were combined with DVC and image analysis to extract the full-field displacements and elastic crystal strains. The displacement fields have been analysed using the developed methods to extract the critical strain energy release rate for crack propagation. Non-linear properties described the effect of microcracking on the elastic modulus in the fracture process zone. The analysis was verified by comparison of the predicted and measured elastic strain fields.

Optical diffraction tomography (ODT) is a tomographic technique that can be used to measure the threedimensional (3D) refractive index distribution within living cells without the requirement of any marker. In principle, ODT can be regarded as a generalization of optical projection tomography which is equivalent to computerized tomography (CT). Both optical tomographic techniques require projection-phase images of cells measured at multiple angles. However, the reconstruction of the 3D refractive index distribution post-measurement differs for the two techniques. It is known that ODT yields better results than projection tomography, because it takes into account diffraction of the imaging light due to the refractive index structure of the sample. Here, we apply ODT to biological cells in a micro uidic chip which combines optical trapping and microfluidic flow to achieve an optofluidic single-cell rotation. In particular, we address the problem that arises when the trapped cell is not rotating about an axis perpendicular to the imaging plane, but instead about an arbitrarily tilted axis. In this paper we show that the 3D reconstruction can be improved by taking into account such a tilted rotational axis in the reconstruction process.

This dissertation presents a contribution to quantitative microwave imaging for breast tumor detection. The study made in the frame of a joint supervision Ph.D. thesis between University Paris-SUD 11 (France) and Mälardalen University (Sweden), has been conducted through two experimental microwave imaging setups, the existing 2.45 GHz planar camera (France) and the multi-frequency flexible robotic system, (Sweden), under development. In this context a 2D scalar flexible numerical tool based on a Newton-Kantorovich (NK) scheme, has been developed. Quantitative microwave imaging is a three dimensional vectorial nonlinear inverse scattering problem, where the complex permittivity of an object is reconstructed from the measured scattered field, produced by the object. The NK scheme is used in order to deal with the nonlinearity and the ill-posed nature of this problem. A TM polarization and a two dimensional medium configuration have been considered in order to avoid its vectorial aspect. The solution is found iteratively by minimizing the square norm of the error with respect to the scattered field data. Consequently, the convergence of such iterative process requires, at least two conditions. First, an efficient calibration of the experimental system has to be associated to the minimization of model errors. Second, the mean square difference of the scattered field introduced by the presence of the tumor has to be large enough, according to the sensitivity of the imaging system. The existing planar camera associated to a flexible 2D scalar NK code, are considered as an experimental platform for quantitative breast imaging. A preliminary numerical study shows that the multi-view planar system is quite efficient for realistic breast tumor phantoms, according to its characteristics (frequency, planar geometry and water as a coupling medium), as long as realistic noisy data are considered. Furthermore, a multi-incidence planar system, more appropriate in term of antenna-array arrangement, is proposed and its concept is numerically validated. On the other hand, an experimental work which includes a new fluid-mixture for the realization of a narrow band cylindrical breast phantom, a deep investigation in the calibration process and model error minimization, is presented. This conducts to the first quantitative reconstruction of a realistic breast phantom by using multi-view data from the planar camera. Next, both the qualitative and quantitative reconstruction of 3D inclusions into the cylindrical breast phantom, by using data from all the retina, are shown and discussed. Finally, the extended work towards the flexible robotic system is presented. / A dissertation prepared through an international convention for a joint supervision thesis with Université Paris-SUD 11, France / Microwaves in biomedicine

Title: Structure analysis of some transition metal silicides using X-ray diffraction and dynamical refinement against electron diffraction data Author: Cinthia Antunes Corrˆea Department: Physics of Materials Supervisor: prof. RNDr. Miloš Janeček, CSc., Department of Physics of Materials Abstract: This thesis presents the crystal structure analysis of several transition metal silicides. The crystal structures were studied primarily by precession electron diffraction tomography (PEDT) employing the dynamical refinement, a method recently developed for accurate crystal structure refinement of electron diffraction data. The optimal values of the parameters of the method were proposed based on the comparison between the dynamical refinement of PEDT data and a high- quality reference structure. We present the results of the comparison using a Ni2Si nanowire with the diameter of 15 nm. The average atomic distance between the model obtained by the dynamical refinement on PEDT data and the one by single crystal X-ray diffraction was 0.006 ˚A. Knowing the accuracy and limitations of the method, the crystal structure of Ni3Si2 was redetermined on a nanowire with 35 nm of diameter. The model obtained had an average error in the atomic posi- tions of 0.006 ˚A. These results show that the accuracy achieved by the dynamical...

The focus of the thesis is on the development of a few stochastic search schemes for inverse problems and their applications in medical imaging. After the introduction in Chapter 1 that motivates and puts in perspective the work done in later chapters, the main body of the thesis may be viewed as composed of two parts: while the first part concerns the development of stochastic search algorithms for inverse problems (Chapters 2 and 3), the second part elucidates on the applicability of search schemes to inverse problems of interest in tomographic imaging (Chapters 4 and 5). The chapter-wise contributions of the thesis are summarized below. Chapter 2 proposes a Monte Carlo stochastic filtering algorithm for the recursive estimation of diffusive processes in linear/nonlinear dynamical systems that modulate the instantaneous rates of Poisson measurements. The same scheme is applicable when the set of partial and noisy measurements are of a diffusive nature. A key aspect of our development here is the filter-update scheme, derived from an ensemble approximation of the time-discretized nonlinear Kushner Stratonovich equation, that is modified to account for Poisson-type measurements. Specifically, the additive update through a gain-like correction term, empirically approximated from the innovation integral in the filtering equation, eliminates the problem of particle collapse encountered in many conventional particle filters that adopt weight-based updates. Through a few numerical demonstrations, the versatility of the proposed filter is brought forth, first with application to filtering problems with diffusive or Poisson-type measurements and then to an automatic control problem wherein the exterminations of the associated cost functional is achieved simply by an appropriate redefinition of the innovation process. The aim of one of the numerical examples in Chapter 2 is to minimize the structural response of a duffing oscillator under external forcing. We pose this problem of active control within a filtering framework wherein the goal is to estimate the control force that minimizes an appropriately chosen performance index. We employ the proposed filtering algorithm to estimate the control force and the oscillator displacements and velocities that are minimized as a result of the application of the control force. While Fig. 1 shows the time histories of the uncontrolled and controlled displacements and velocities of the oscillator, a plot of the estimated control force against the external force applied is given in Fig. 2. (a) (b) Fig. 1. A plot of the time histories of the uncontrolled and controlled (a) displacements and (b) velocities. Fig. 2. A plot of the time histories of the external force and the estimated control force Stochastic filtering, despite its numerous applications, amounts only to a directed search and is best suited for inverse problems and optimization problems with unimodal solutions. In view of general optimization problems involving multimodal objective functions with a priori unknown optima, filtering, similar to a regularized Gauss-Newton (GN) method, may only serve as a local (or quasi-local) search. In Chapter 3, therefore, we propose a stochastic search (SS) scheme that whilst maintaining the basic structure of a filtered martingale problem, also incorporates randomization techniques such as scrambling and blending, which are meant to aid in avoiding the so-called local traps. The key contribution of this chapter is the introduction of yet another technique, termed as the state space splitting (3S) which is a paradigm based on the principle of divide-and-conquer. The 3S technique, incorporated within the optimization scheme, offers a better assimilation of measurements and is found to outperform filtering in the context of quantitative photoacoustic tomography (PAT) to recover the optical absorption field from sparsely available PAT data using a bare minimum ensemble. Other than that, the proposed scheme is numerically shown to be better than or at least as good as CMA-ES (covariance matrix adaptation evolution strategies), one of the best performing optimization schemes in minimizing a set of benchmark functions. Table 1 gives the comparative performance of the proposed scheme and CMA-ES in minimizing a set of 40-dimensional functions (F1-F20), all of which have their global minimum at 0, using an ensemble size of 20. Here, 10 5 is the tolerance limit to be attained for the objective function value and MAX is the maximum number of iterations permissible to the optimization scheme to arrive at the global minimum. Table 1. Performance of the SS scheme and Chapter 4 gathers numerical and experimental evidence to support our conjecture in the previous chapters that even a quasi-local search (afforded, for instance, by the filtered martingale problem) is generally superior to a regularized GN method in solving inverse problems. Specifically, in this chapter, we solve the inverse problems of ultrasound modulated optical tomography (UMOT) and diffraction tomography (DT). In UMOT, we perform a spatially resolved recovery of the mean-squared displacements, p r of the scattering centres in a diffusive object by measuring the modulation depth in the decaying autocorrelation of the incident coherent light. This modulation is induced by the input ultrasound focussed to a specific region referred to as the region of interest (ROI) in the object. Since the ultrasound-induced displacements are a measure of the material stiffness, in principle, UMOT can be applied for the early diagnosis of cancer in soft tissues. In DT, on the other hand, we recover the real refractive index distribution, n r of an optical fiber from experimentally acquired transmitted intensity of light traversing through it. In both cases, the filtering step encoded within the optimization scheme recovers superior reconstruction images vis-à-vis the GN method in terms of quantitative accuracies. Fig. 3 gives a comparative cross-sectional plot through the centre of the reference and reconstructed p r images in UMOT when the ROI is at the centre of the object. Here, the anomaly is presented as an increase in the displacements and is at the centre of the ROI. Fig. 4 shows the comparative cross-sectional plot of the reference and reconstructed refractive index distributions, n r of the optical fiber in DT. Fig. 3. Cross-sectional plot through the center of the reference and reconstructed p r images. Fig. 4. Cross-sectional plot through the center of the reference and reconstructed n r distributions. In Chapter 5, the SS scheme is applied to our main application, viz. photoacoustic tomography (PAT) for the recovery of the absorbed energy map, the optical absorption coefficient and the chromophore concentrations in soft tissues. Nevertheless, the main contribution of this chapter is to provide a single-step method for the recovery of the optical absorption field from both simulated and experimental time-domain PAT data. A single-step direct recovery is shown to yield better reconstruction than the generally adopted two-step method for quantitative PAT. Such a quantitative reconstruction maybe converted to a functional image through a linear map. Alternatively, one could also perform a one-step recovery of the chromophore concentrations from the boundary pressure, as shown using simulated data in this chapter. Being a Monte Carlo scheme, the SS scheme is highly parallelizable and the availability of such a machine-ready inversion scheme should finally enable PAT to emerge as a clinical tool in medical diagnostics. Given below in Fig. 5 is a comparison of the optical absorption map of the Shepp-Logan phantom with the reconstruction obtained as a result of a direct (1-step) recovery. Fig. 5. The (a) exact and (b) reconstructed optical absorption maps of the Shepp-Logan phantom. The x- and y-axes are in m and the colormap is in mm-1. Chapter 6 concludes the work with a brief summary of the results obtained and suggestions for future exploration of some of the schemes and applications described in this thesis.

A procedure to evaluate the leaching properties of radionuclides from irradiated graphite waste has been developed by combining ANSI 16.1 (USA) and NEN 7345 (Netherlands) standardised diffusion leaching techniques. The ANSI 16.1 standard has been followed to the acquire the leachates and to determine the leach rate/ diffusion coefficient and NEN 7345 standard technique has been used to determine the diffusion mechanism of radionuclides. The investigation employs simulated Drigg groundwater as a leachant using semi-dynamic technique for the production of leachate specimens. From gamma spectroscopy analysis the principal radionuclides present in terms of activity were 60Co, 137Cs, 134Cs, 155Eu, 133Ba and 46Sc. The dominant radionuclides are 60Co, 134Cs and 133Ba which together account for about 91 % of the total activity. The 91 % can be broken down into 73.4 % 60Co, 9.1 % 134Cs and 8.1 % 133Ba. Analysis of total beta and total beta without tritium activity release from Magnox graphite was measured using liquid scintillating counting. Preliminary results show that there is an initial high release of activity and decreases when the leaching period increases. This may be due to the depletion of contaminants which were absorbed by the internal pore networks and the surface. During the leaching test approximately 275.33 ± 18.20 Bq of 3H and 106.26 ± 7.01 Bq of 14C was released into the leachant within 91 days. Irradiation induced damages to the nuclear graphite crystal structure have been shown to cause disruption of the bonding across the basal planes. Moreover, the closures of Mrozowski cracks have been observed in nuclear graphite, the bulk property are governed by the porosity, in particular, at the nanometre scale. Therefore, knowledge of the crystallite structure and porosity distribution is very important; as it will assist in understand the affects of irradiated damage and location and the mechanism of the leaching of radionuclides. The work reported herein contributed several key findings to the international work on graphite leaching to offer guidance leading toward obtaining leaching data in the future: (a) the effective diffusion coefficient for 14C from graphite waste has been determined. The diffusion process for 14C has two stages resulting two different values of diffusion coefficient, i.e., for the fast and slow components; (b) the controlling leaching mechanism for 3H radionuclide from graphite is shown to be surface wash–off; and for that of 14C radionuclide the initial controlling leaching mechanism is surface wash-off following by diffusion which is the major transport mechanism ; (c) The weight loss originates from the open pore structure which has been opened up by radiolytic oxidation; at the higher weight losses much of the closed porosity in the graphite has been opened. The investigation indicates that weigh loss has a major influence on the leaching of elements from the irradiated graphite; and (d) the analysis of the pores in nuclear graphite can be categorised into three types. These three types of pores are: (1) small pores narrow which are slit-shaped pores in the binder phase or matrix, (2) gas evolution pores or gas entrapment pores within the binder phase or matrix and (3) lenticular pores which are large cracks within the filler particles. It is shown in this thesis that by using tomography to study the morphology of the different pores coupled with the distribution of impurities an understanding of the role of porosity in leaching is possible.

[ES] Las zeolitas son materiales cristalinos microporosos con canales y tamaños de poro de dimensiones moleculares. La estructura y composición de las zeolitas les confiere interesantes propiedades que permiten su aplicación en una amplia gama de aplicaciones industriales como adsorción, separación o catálisis. La síntesis de zeolitas es la etapa más importante para el control de la estructura y composición de las zeolitas y, por tanto, crítica para la optimización de sus propiedades. Esta tesis se ha centrado en la síntesis de zeolitas utilizando compuestos que contienen fósforo (cationes fosfonio y aminofosfonio) como Agentes Directores de Estructura (P-ADE). El uso de compuestos fosforados influye en la cristalización y propiedades de las zeolitas obtenidas en comparación con las zeolitas obtenidas con cationes de amonio clásicos. Los compuestos fosforados se eligieron debido a su diferente química y estabilidad con respecto a los cationes de amonio clásicos comúnmente usados en la síntesis de zeolitas. Estos aspectos se estudiaron con un estudio comparativo de diferentes cationes de amonio y fosforados. Los compuestos de fósforo utilizados en este trabajo han dado lugar a nuevas estructuras cristalinas (ITQ-58 e ITQ-66) y han abierto nuevas vías de síntesis de zeolitas ya conocidas (RTH, IWV y DON), ampliando su gama de composiciones químicas. La descomposición térmica de los P-ADE confinados dentro de las zeolitas da lugar a la formación de especies de fósforo extra-red que permanecen dentro de los canales y cavidades de las zeolitas. Estas especies modulan las propiedades ácidas y de adsorción de los materiales finales dependiendo de los tratamientos post-síntesis. En este trabajo se ha estudiado una ruta para la incorporación de cantidades controladas de fósforo durante la etapa de síntesis. Esto ha permitido controlar la adsorción y las propiedades ácidas en las zeolitas de poro pequeño, lo que no se puede lograr mediante metodologías de post-síntesis. / [CA] Les zeolites són materials cristal·lins microporosos amb canals i mides de porus de dimensions moleculars. L'estructura i composició de les zeolites els confereix interessants propietats que permeten la seua aplicació en una àmplia gamma d'aplicacions industrials com adsorció, separació o catàlisi. La síntesi de zeolites és l'etapa més important per al control de l'estructura i composició de les zeolites i, per tant, crítica per a l'optimització de les seues propietats. Aquesta tesi s'ha centrat en la síntesi de zeolites utilitzant compostos que contenen fòsfor (cations fosfoni i aminofosfoni) com a agents directors d'estructura (P-ADE). L'ús de compostos fosforats influeix en la cristal·lització i propietats de les zeolites obtingudes en comparació amb les zeolites obtingudes amb cations d'amoni clàssics. Els compostos fosforats es van triar a causa de la seua diferent química i estabilitat pel que fa als cations d'amoni clàssics utilitzats en la síntesi de zeolites. Aquests aspectes s¿estudiaren amb un estudi comparatiu de diferents cations d'amoni i fosforats. Els compostos de fòsfor utilitzats en aquest treball han donat lloc a noves estructures cristal·lines (ITQ-58 i ITQ-66) i han obert noves vies de síntesi de zeolites ja conegudes (RTH, IWV i DO), ampliant la seua gamma de composicions químiques. La descomposició tèrmica dels P-ADE atrapats dins de les zeolites dona lloc a la for-mació d'espècies de fòsfor extra-xarxa que romanen dins dels canals i cavitats de les zeolites. Aquestes espècies modulen les propietats àcides i d'adsorció dels materials finals depenent dels tractaments post-síntesi. En aquest treball s'ha estudiat una ruta per la incorporació de quantitats controlades de fòsfor durant l'etapa de síntesi. Això ha permés controlar l'adsorció i les propietats àcides en les zeolites de porus petit, el que no es pot aconseguir mitjançant metodologies de post-síntesi. / [EN] Zeolites are microporous crystalline materials with channels and pore openings of molecular dimensions. The structure and composition of zeolites confers them interesting properties that allow their application in a wide range of industrial applications as adsorption, separation or catalysis. The synthesis of zeolites is the most important stage to control the structure and composition of zeolites, and thus, critical to optimize their properties. This thesis has been focused on the synthesis of zeolites using phosphorous containing compounds (phosphonium and aminophosphonium cations) as Organic Structure Directing Agents (P-OSDA). The use of these phosphorous compounds influence the crystallization and properties of the obtained zeolites compared to zeolites obtained with classical ammo-nium cations. Phosphorous compounds were chosen because of their different chemistry and stabil-ity properties respect to classical ammonium cations commonly used in the synthesis of zeo-lites. These aspects were studied in a comparative study with different ammonium and phosphorous cations. The phosphorous compounds used in this work have yielded new crystalline structures (ITQ-58 and ITQ-66) and opened new routes for the synthesis of already known zeolites (RTH, IWV and DON), widening their chemical composition range. The thermal decomposition of the P-OSDAs entrapped inside the zeolites yields to the formation of extra-framework phosphorus species that remain inside the channels and voids of the zeolites. These species modulate the adsorption and acid properties of the final materials depending on the post-synthesis treatments. In this work, a route for the incorporation of controlled amounts of phosphorus during the synthesis stage has been studied. This has allowed to control the adsorption and acid properties in small pores zeolites, which cannot be achieved by post-synthesis methodologies. / I wish to firstly acknowledge the Spanish Government for the necessary funding for the FPI pre-doctoral fellowship (BES-2013-062999). Also, this thesis would not have been possible without the infrastructures provided by the UPV and the CSIC staff, fused into the ITQ. Furthermore, I want to acknowledge the Microscopy Service of the UPV for their support in sample microscopy characterization / Simancas Coloma, J. (2021). Synthesis and Characterization of Zeolitic Materials Using Phosphorous Organic Structure Directing Agents [Tesis doctoral]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/171267 / TESIS